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2,2-Dimethoxypropane → HCID 86733713, 화합물

HRID 918271
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HRID 918271 반응식
[CH3:1][O:2][C:3]1[CH:4]=[C:5]2[C:10](=[CH:11][CH:12]=1)[CH2:9][CH:8]([C@H:13]1[C@:17]([CH3:22])([CH2:18][C:19]([OH:21])=[O:20])[C@@H:16]([OH:23])[CH2:15][CH2:14]1)[CH2:7][CH2:6]2.[CH3:24]OC(OC)(C)C.O.C1(C)C=CC(S(O)(=O)=O)=CC=1>CO>[CH3:1][O:2][C:3]1[CH:4]=[C:5]2[C:10](=[CH:11][CH:12]=1)[CH2:9][CH:8]([C@H:13]1[C@:17]([CH3:22])([CH2:18][C:19]([O:21][CH3:24])=[O:20])[C@@H:16]([OH:23])[CH2:15][CH2:14]1)[CH2:7][CH2:6]2
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 64952,2-DimethoxypropaneHCID 521998p-Toluenesulfonic acid monohydrateHCID 68145100HCID 68145100, 화합물

생성물 1

HCID 86733713HCID 86733713, 화합물

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

A solution of 2.19 g of (1S,2S,5S)-5-(1,2,3,4-tetrahydro-6-methoxy-2-naphthyl)-2-hydroxy-1-methylcyclo-pentaneacetic acid and 5 ml of 2,2-dimethoxypropane in 40 ml of methanol containing 0.05 g of p-toluenesulfonic acid monohydrate is refluxed for 18 hours. The resultant solution is partitioned between aqueous 5% sodium bicarbonate and ether. The ether phase is separated, dried over magnesium sulfate, and stripped of solvent by vacuum distillation. The residue is crystallized from a mixture of acetone and hexane to give methyl (1S,2S,5S)-5-(1,2,3,4-tetrahydro-6-methoxy-2-naphthyl)-2-hydroxy-1-methylcyclopentaneacetate melting at approximately 86°-87°.

후처리

  1. customThe resultant solution is partitioned between aqueous 5% sodium bicarbonate and ether
  2. customThe ether phase is separated
  3. dry with materialdried over magnesium sulfate
  4. distillationstripped of solvent by vacuum distillation
  5. customThe residue is crystallized from a mixture of acetone and hexane

출처 및 근거

ORD 기록
ord-7a623c1b0c0f42c1a1c92eb8b618fe3c
출처 데이터셋
uspto-grants-1976_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US03970686

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